US8691722B2 - Sorbent comprising activated carbon particles, sulfur and metal catalyst - Google Patents
Sorbent comprising activated carbon particles, sulfur and metal catalyst Download PDFInfo
- Publication number
- US8691722B2 US8691722B2 US12/167,418 US16741808A US8691722B2 US 8691722 B2 US8691722 B2 US 8691722B2 US 16741808 A US16741808 A US 16741808A US 8691722 B2 US8691722 B2 US 8691722B2
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- US
- United States
- Prior art keywords
- sulfur
- process according
- sorbent
- metal
- binder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related, expires
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 106
- 239000002184 metal Substances 0.000 title claims abstract description 104
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 239000002594 sorbent Substances 0.000 title claims abstract description 101
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 79
- 239000011593 sulfur Substances 0.000 title claims abstract description 79
- 239000003054 catalyst Substances 0.000 title claims abstract description 66
- 239000002245 particle Substances 0.000 title claims abstract description 34
- 239000011230 binding agent Substances 0.000 claims description 70
- 239000000203 mixture Substances 0.000 claims description 68
- 238000000034 method Methods 0.000 claims description 44
- 230000008569 process Effects 0.000 claims description 31
- 229920005989 resin Polymers 0.000 claims description 31
- 239000011347 resin Substances 0.000 claims description 31
- 150000001875 compounds Chemical class 0.000 claims description 26
- 230000003647 oxidation Effects 0.000 claims description 20
- 238000007254 oxidation reaction Methods 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- 238000001125 extrusion Methods 0.000 claims description 9
- 229910052976 metal sulfide Inorganic materials 0.000 claims description 9
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
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- B01D2255/2045—Calcium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/2073—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20761—Copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20769—Molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20776—Tungsten
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
Definitions
- This disclosure relates to sorbents comprising activated carbon particles, sulfur, and metal catalyst.
- the sorbents may be used, for example, for the removal of a contaminant, such as mercury, from a fluid stream.
- Hazardous contaminant emissions have become environmental issues of increasing concern because of the potential dangers posed to human health. For instance, coal-fired power plants and medical waste incineration are major sources of human activity related mercury emission into the atmosphere.
- a technology currently in use for controlling emissions of elemental mercury as well as oxidized mercury is activated carbon injection (ACI).
- ACI activated carbon injection
- the ACI process involves injecting activated carbon powder into a flue gas stream and using a fabric filter or electrostatic precipitator to collect the activated carbon powder that has sorbed mercury.
- ACI technologies generally require a high C:Hg ratio to achieve the desired mercury removal level (>90%), which results in a high portion cost for sorbent material.
- the high C:Hg ratio indicates that ACI does not utilize the mercury sorption capacity of carbon powder efficiently.
- the inventors have now discovered new sorbents for the removal of contaminants such as mercury from fluids.
- FIG. 1 is an SEM image of a sorbent according to one embodiment.
- sulfur in any oxidation state, as elemental sulfur or in a chemical compound or moiety comprising sulfur
- a metal catalyst in any oxidation state, as elemental metal or in a chemical compound or moiety comprising the metal.
- the activated carbon particles may be, for example, activated carbon powder, granular activated carbon, or a combination thereof.
- exemplary activated carbon particles include those having a median size of from 1 to 100 microns.
- the sulfur may include sulfur at any oxidation state, including elemental sulfur (0), sulfate (+6), sulfite (+4), and sulfide ( ⁇ 2).
- the term sulfur thus includes elemental sulfur or sulfur present in a chemical compound or moiety.
- the amount of sulfur present in the sorbent can be selected depending on the particular metal catalyst also present, application for which the sorbent is used, and the desired contaminant removing capacity and efficiency of the sorbent.
- the sorbent comprises from 1% to 20% by weight of sulfur, or from 1% to 15%, from 3% to 8%, from 2% to 10%, from 0.1 to 5%, or from 2 to 5% by weight of sulfur.
- the weight percent of sulfur is calculated on the basis of elemental sulfur, with any sulfur in other states converted to elemental state for the purpose of calculating the total amount of sulfur in the sorbent.
- the metal catalyst includes any metal element in any oxidation state, as elemental metal or in a chemical compound or moiety comprising the metal, which is in a form that promotes the removal of a contaminant (such as cadmium, mercury, chromium, lead, barium, beryllium, nickel, cobalt, vanadium, zinc, copper, manganese, antimony, silver, thallium, arsenic or selenium) from a fluid in contact with the sorbent.
- Metal elements can include alkali metals, alkaline earth metals, transition metals, rare earth metals (including lanthanoids), and other metals such as aluminum, gallium, indium, tin, lead, thallium and bismuth.
- the metal catalysts can exist at any valency.
- iron it may be present at +3, +2 or 0 valencies or as mixtures of differing valencies, and can be present as metallic iron (0), or in FeO, Fe 2 O 3 , Fe 3 O 8 , FeS, FeCl 2 , FeCl 3 , FeSO 4 , and the like.
- manganese it may be present at +4, +2 or 0 valencies or as mixtures of differing valencies, and can be present as metallic manganese (0), or in MnO, MnO 2 , MnS, MnCl 2 , MnCl 4 , MnSO 4 , and the like.
- the metal catalyst is an alkali metal such as lithium, sodium, or potassium. In other embodiments, the metal catalyst is an alkaline earth metal such as magnesium, calcium, or barium. In other embodiments, the metal catalyst is a transition metal, such as palladium, platinum, silver, gold, manganese, or iron. In other embodiments, the metal catalyst is a rare earth metal such as cerium. In some embodiments, the metal catalyst is in elemental form. In other embodiments, the metal catalyst is present in a metal sulfide. In other embodiments, the metal catalyst is present in a transition metal sulfide or oxide.
- the sorbent body comprises at least one catalyst other than an alkali metal, an alkaline earth metal, or transition metal, or other than a metal oxide.
- the sorbent body comprises at least one catalyst other than sodium, other than potassium, other than magnesium, other than calcium, other than aluminum, other than titanium, other than zirconium, other than chromium, other than magnesium, other than iron and/or other than zinc.
- the sorbent body comprises at least one metal catalyst other than aluminum, vanadium, iron, cobalt, nickel, copper, or zinc, either in elemental form or as sulfates.
- the amount of the metal catalyst present in the sorbent can be selected depending on the particular metal catalyst used, application for which the sorbent is used, and the desired contaminant removing capacity and efficiency of the sorbent. In certain embodiments, the amount of the metal catalyst ranges from 1% to 25% by weight, from 1-20%, from 1-15%, from 2% to 18%, from 3-10%, from 3-5%, from 5% to 15%, or from 5% to 10% by weight of the sorbent.
- the weight percent of metal catalyst is calculated on the basis of elemental metal, with any metal in other states converted to elemental state for the purpose of calculation of the total amount of metal catalyst in the relevant material.
- Metal elements present in an inert from, such as in an inorganic binder compound, are not considered metal catalysts and do not contribute to the weight percent of a metal catalyst.
- the amount of sulfur or metal catalyst may be determined using any appropriate analytical technique, such as mass spectroscopy and LECO analysis (for sulfur).
- the metal catalyst can function in one or more of the following ways to promote the removal of a contaminant from a fluid in contact with the sorbent: (i) temporary or permanent chemical sorption (e.g., via covalent and/or ionic bonds) of a contaminant; (ii) temporary or permanent physical sorption of a contaminant; (iii) catalyzing the reaction/sorption of a contaminant with other components of the sorbent body; (iv) catalyzing the reaction of a contaminant with the ambient atmosphere to convert it from one form to another for sorption; (v) trapping a contaminant already sorbed by other components of the sorbent body; and (vi) facilitating the transfer of a contaminant to the active sorbing sites.
- temporary or permanent chemical sorption e.g., via covalent and/or ionic bonds
- At least a portion of the sulfur, of the metal catalyst, or of both the sulfur and metal catalyst is in a state capable of chemically bonding with cadmium, mercury, chromium, lead, barium, beryllium, nickel, cobalt, vanadium, zinc, copper, manganese, antimony, silver, thallium, arsenic or selenium.
- at least a portion of the sulfur can be in a state capable of chemically bonding with mercury.
- At least a portion of the metal catalyst is chemically bound to at least a portion of the sulfur.
- the term “at least a portion” in this and other contexts refers to some or all of the material being described.
- some or all of the metal catalyst in the sorbent can be chemically bound to some or all of the sulfur in the sorbent.
- at least a portion of the sulfur is chemically bound to at least a portion of carbon in the activated carbon particles.
- the sorbent comprises a metal sulfide.
- metal sulfides include sulfides of manganese, copper, calcium, palladium, molybdenum, or tungsten, and combinations thereof.
- the metal element in the metal sulfide is not limited to those examples.
- the metal element in the metal sulfides may be selected from alkali metals, alkaline earth metals, transition metals, rare earth metals (including lanthanoids), and other metals such as aluminum, gallium, indium, tin, lead, thallium and bismuth.
- the sorbent comprises a metal bound to sulfur (such as a metal sulfide), or where the sorbent comprises sulfur bound to carbon
- the sorbent further comprises additional sulfur such as elemental sulfur.
- at least a portion of sulfur is not bound to metal catalyst and/or at least a portion of metal catalyst is not bound to sulfur.
- the sorbent of the embodiments described above further comprise a discontinuous binder providing a bond between the activated carbon particles.
- discontinuous refers to the binder serving to adhere or bind activated carbon particles without the binder itself being in the form of a supporting matrix for the activated carbon particles. The mechanical strength and durability of the sorbent is therefore attributable to the bound activated carbon particles rather than to a supporting binder matrix.
- FIG. 1 is an SEM image of a sorbent according to one embodiment of the invention.
- the image illustrates activated carbon particles, such as activated carbon particle 110 , and inorganic material, such as inorganic materials 120 .
- the image shows that the sorbent does not contain a matrix of binder supporting the activated carbon particles, but instead any binder is in a discontinuous form, such as in particulate form.
- the total amount of binder present in the sorbent is an amount up to 30 wt %, up to 25 wt %, up to 20 wt %, up to 15 wt %, up to 10 wt %, or up to 5 wt %.
- these wt % values represent the wt % of an organic binder.
- these wt % values represent the wt % of an inorganic binder.
- the sorbent of the invention comprises up to 30 wt % of inorganic binder.
- the sorbent comprises up to 20 wt % of organic binder.
- the binder may comprise an inorganic binder or an organic binder.
- binder includes one binder as well as combinations of two or more binders, each independently being an inorganic binder or inorganic binder.
- the sorbent can comprise both an inorganic binder and an organic binder, or two or more inorganic binders or two or more organic binders.
- Exemplary inorganic binders include certain oxides, sulfates, carbonates, and phosphates, such as certain oxides, sulfates, carbonates, and phosphates of metals or of semi-metals such as silicon and germanium. For instance, talc, clay such as bentonite clay, and Plaster of Paris may be used as inorganic binders.
- any metal element in the inorganic binder material is chemically and physically inert, meaning that it does not catalyze the sorption of contaminants onto sorbents of the invention.
- the sorbents may also comprise organic binders.
- organic binder includes not only organic compounds but also the carbon remnants of such compounds if they have been carbonized by exposure to carbonization conditions such as a high temperature. Thus, reference to a particular material as an “organic binder” includes that material as well as the carbonized remnants of such a material.
- One embodiment includes organic binder that has not been carbonized, while another embodiment includes organic binder that has been carbonized.
- Exemplary organic binders include organic resins.
- Organic resins include thermosetting resins and thermoplastic resins (e.g., polyvinylidene chloride, polyvinyl chloride, polyvinyl alcohol, and the like).
- Synthetic polymeric material may be used, such as phenolic resins or a furfural alcohol based resin such as furan resins.
- Exemplary suitable phenolic resins are resole resin such as plyophen resin.
- An exemplary suitable furan liquid resin is Furcab-LP from QO Chemicals Inc., Ind., U.S.A.
- An exemplary solid resin is solid phenolic resin or novolak. Any organic resin binder may be uncured, cured, or carbonized in the sorbents of the invention.
- the sorbent does not comprise a ceramic binder. In other embodiments, the sorbent does not comprise carbon or activated carbon binder.
- the sorbent may comprise cellulose compounds.
- Cellulose compounds include cellulose ethers, such as methylcellulose, ethylhydroxy ethylcellulose, hydroxybutylcellulose, hydroxybutyl methylcellulose, hydroxyethylcellulose, hydroxymethylcellulose, hydroxypropylcellulose, hydroxypropyl methylcellulose, hydroxyethyl methylcellulose, sodium carboxy methylcellulose, and mixtures thereof.
- An example methylcellulose binder is METHOCEL A, sold by the Dow Chemical Company.
- Example hydroxypropyl methylcellulose binders include METHOCEL E, F, J, K, also sold by the Dow Chemical Company.
- METHOCEL A4M is an example binder for use with a RAM extruder.
- METHOCEL F240C is an example binder for use with a twin screw extruder.
- sulfur in any oxidation state, as elemental sulfur or in a chemical compound or moiety comprising sulfur
- a metal catalyst in any oxidation state, as elemental metal or in a chemical compound or moiety comprising the metal
- the binder in this instance may or may not be of a discontinuous form.
- the activated carbon, sulfur, metal catalyst and binder may be selected from those materials described previously.
- the extent of any binding between sulfur and metal catalyst may be controlled by selection of appropriate relative amounts of sulfur and metal catalyst used to make the sorbent as well as selection of processing conditions for making the sorbent.
- sulfur in any oxidation state, as elemental sulfur or in a chemical compound or moiety comprising sulfur
- a metal catalyst in any oxidation state, as elemental metal or in a chemical compound or moiety comprising the metal
- the binder in this instance may or may not be of a discontinuous form.
- the activated carbon, sulfur, metal catalyst and binder may be selected from those materials described previously.
- the distribution of sulfur and/or metal catalyst within the activated carbon particle bodies may be controlled by, for example, homogenous in-situ incorporation of sulfur and/or metal catalyst in precursor material used to form the activated carbon particles.
- the sorbents of any embodiments discussed above may be in any appropriate physical form.
- the sorbent is in the form of a granule, pellet, or planar or tubular structure.
- the sorbent is in the form of a monolith.
- the sorbent is in the form of a flow-through sorbent body, such as in the form of a honeycomb.
- Exemplary flow-through sorbents include, for example, any structure comprising channels, porous networks, or any other passages that would permit the flow of a fluid stream through the sorbent.
- the flow-through sorbent may be a monolith or an arrangement of interconnected structures creating openings through which a fluid steam may pass.
- the flow-through sorbent may be a honeycomb sorbent comprising an inlet end, an outlet end, and a multiplicity of cells extending from the inlet end to the outlet end, the cells being defined by intersecting porous cell walls.
- a honeycomb sorbent could optionally comprise one or more selectively plugged honeycomb cell ends to provide a wall flow-through structure that allows for more intimate contact between a fluid stream and cell walls.
- the cell density of a honeycomb can be adjusted during an extrusion process to achieve desired physical attributes.
- the cell density of the honeycomb can range from 25 to 500 cells ⁇ inch ⁇ 2 (3.88 to 77.5 cells ⁇ cm ⁇ 2 ) in certain embodiments, from 50 to 200 cells ⁇ inch ⁇ 2 (7.75 to 31.0 cells ⁇ cm ⁇ 2 ) in certain other embodiments, and from 50 to 100 cells ⁇ inch ⁇ 2 (7.75 to 15.5 cells ⁇ cm ⁇ 2 ) in certain other embodiments.
- the thickness of the cell walls ranges from 1 mil to 50 mil, for example from 10 mil to 30 mil.
- the sorbent is provided as a coating on an inorganic substrate.
- exemplary inorganic substrates include glass, glass-ceramic, ceramic, and metal substrates.
- Some example substrate materials include cordierite, mullite, clay, magnesia, metal oxides, talc, zircon, zirconia, zirconates, zirconia-spinel, magnesium alumino-silicates, spinel, alumina, silica, silicates, borides, alumino-silicates, e.g., porcelains, lithium aluminosilicates, alumina silica, feldspar, titania, fused silica, nitrides, borides, carbides, e.g., silicon carbide, silicon nitride or combinations of these.
- the inorganic substrates may comprise one or more coatings of inorganic material, which may also be porous. Coatings of inorganic material may be provided as washcoats of inorganic material.
- Exemplary inorganic coating materials include cordierite, alumina (such as alpha-alumina and gamma-alumina), mullite, aluminum titanate, titania, zirconia, and ceria particles and combinations thereof.
- the inorganic substrate may itself be, for example, be in the form of a flow-through structure, such as a honeycomb.
- Exemplary flow-through structures include, for example, any structure comprising channels, porous networks, or any other passages that would permit the flow of a fluid stream through the structure.
- the inorganic substrate may also be in the form of, for example, granules, pellets, or planar or tubular structures.
- a coating of the sorbent may coat all or a portion of the surface of the inorganic substrate, and may impregnate the substrate to some extent if the surface of the substrate is porous.
- the coating may coat the inner channel surfaces of an inorganic honeycomb substrate and any outer surfaces of the honeycomb.
- Sorbents of the invention may be formed by any suitable technique.
- a sorbent body may be made by a first process that comprises:
- the activated carbon, sulfur, metal catalyst and binder may be selected from the materials discussed above in the context of the sorbents of the invention.
- the metal catalyst may be in a form selected from: (i) halides and oxides of alkali and alkaline earth metals; (ii) precious metals and compounds thereof; (iii) oxides, sulfides, and salts of vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, niobium, molybdenum, silver, tungsten and lanthanoids; or (iv) combinations and mixtures of two or more of (i), (ii) and (iii).
- the metal catalyst may be in a form selected from: (i) oxides, sulfides, sulfates, acetates and salts of manganese; (ii) oxides, sulfides and salts of iron; (iii) combinations of (i) and KI; (iv) combinations of (ii) and KI; and/or (v) mixtures and combinations of any two or more of (i), (ii), (iii) and (iv).
- the sulfur may be in a form selected from, for example, sulfur powder, sulfur-containing powdered resin, sulfides, sulfates, and other sulfur-containing compounds, and mixtures or combination of any two or more of these.
- Exemplary sulfur-containing compounds include hydrogen sulfide and/or its salts, carbon disulfide, sulfur dioxide, thiophene, sulfur anhydride, sulfur halides, sulfuric ester, sulfurous acid, sulfacid, sulfatol, sulfamic acid, sulfan, sulfanes, sulfuric acid and its salts, sulfite, sulfoacid, sulfobenzide, and mixtures thereof.
- the binder comprises an organic resin.
- the organic resin may, for example, be cured after forming the mixture into the shape of a sorbent body. Curing can be performed, for example, in air at atmospheric pressure and typically by heating the structure at a temperature of from 70° C. to 200° C. for about 0.5 to about 5.0 hours.
- the body is heated from a low temperature to a higher temperature in stages, for example, from 70° C., to 90° C., to 125° C., to 150° C., each temperature being held for a period of time.
- curing can also be accomplished by adding a curing additive such as an acid additive at room temperature.
- the mixture can be formed into the shape of a sorbent body by any appropriate technique, such as by extrusion.
- Extrusion can be done by using standard extruders (ram extruder, single-screw, double-screw, and the like) and custom extrusion dies, to make sorbent bodies with various shapes and geometries, such as honeycombs, pellets, rods, spaghetti, and the like. Extrusion is particularly effective for making monolithic honeycomb bodies having a plurality of channels that can serve as fluid passageways.
- Rapid prototyping the automatic construction of physical objects using solid freeform fabrication, may also be used to shape the sorbent.
- Rapid prototyping comprises obtaining a virtual design, for example a computer aided design, converting the design into virtual thin horizontal cross sections, then creating each cross section of the design in physical space, one after the next, until the shape is completed.
- One embodiment includes obtaining a virtual design of a shaped body, converting the design into virtual thin horizontal cross sections, and creating each cross section in physical space from the composition.
- rapid prototyping is 3D printing.
- the formed body may also be optionally dried and optionally fired as well.
- the body can be dried, for example, in an environment at 75-200° C.
- the body can be fired to impart greater mechanical integrity to the structure.
- Exemplary firing conditions include firing at 600° C. to 1500° C. for a period of from 0.5 to 10 hours in a controlled gas environment at a heating rate of, for example, 0.5-2° C./min.
- the firing process can be executed for 20-45 hours at 1100-1300° C. in air or in a mixture of nitrogen and oxygen.
- the structure may be heated to carbonize any organic binder, for example at a temperature of 600° C. or more, then fired at a higher temperature to achieve sintering of inorganic binder material, for instance.
- a second technique for making a sorbent body includes a process that comprises:
- preparation of a homogenous mixture of the carbon source, sulfur and metal catalyst in the first mixture, followed by carbonization can lead to sulfur and metal catalyst being distributed throughout the activated carbon particle bodies.
- the activated carbon, sulfur, metal catalyst, and binder may be selected from the materials discussed above in the context of the sorbents of the invention and the first process for making a sorbent body discussed previously.
- Exemplary carbon sources include synthetic carbon-containing polymeric material, organic resins, charcoal powder, coal tar pitch, petroleum pitch, wood flour, cellulose and derivatives thereof, natural organic materials such as wheat flour, wood flour, corn flour, nut-shell flour, starch, coke, coal, or mixtures or combinations of any two or more of these.
- the carbon source comprises an organic resin.
- organic resins include thermosetting resins and thermoplastic resins (e.g., polyvinylidene chloride, polyvinyl chloride, polyvinyl alcohol, and the like).
- Synthetic polymeric material may be used, such as phenolic resins or a furfural alcohol based resin such as furan resins.
- phenolic resins are resole resins such as plyophen resins.
- An exemplary suitable furan liquid resin is Furcab-LP from QO Chemicals Inc., Ind., U.S.A.
- An exemplary solid resin is solid phenolic resin or novolak.
- the carbon source such as an organic resin
- the first mixture may be carbonized, for instance, by subjecting it to an elevated carbonizing temperature in an O 2 -depleted atmosphere.
- the carbonization temperature can range from 600 to 1200° C., in certain embodiments from 700 to 1000° C.
- the carbonizing atmosphere can be inert, comprising mainly a non reactive gas, such as N 2 , Ne, Ar, mixtures thereof, and the like.
- a non reactive gas such as N 2 , Ne, Ar, mixtures thereof, and the like.
- Such reactions can include, inter alia:
- the first mixture is then activated.
- the carbonized mixture may be activated, for example, in a gaseous atmosphere selected from CO 2 , H 2 O, a mixture of CO 2 and H 2 O, a mixture of CO 2 and nitrogen, a mixture of H 2 O and nitrogen, and a mixture of CO 2 and another inert gas, for example, at an elevated activating temperature in a CO 2 and/or H 2 O-containing atmosphere.
- the atmosphere may be essentially pure CO 2 or H 2 O (steam), a mixture of CO 2 and H 2 O, or a combination of CO 2 and/or H 2 O with an inert gas such as nitrogen and/or argon. Utilizing a combination of nitrogen and CO 2 , for example, may result in cost savings.
- a CO 2 and nitrogen mixture may be used, for example, with CO 2 content as low as 2% or more. Typically a mixture of CO 2 and nitrogen with a CO 2 content of 5-50% may be used to reduce process costs.
- the activating temperature can range from 600° C. to 1000° C., in certain embodiments from 600° C. to 900° C.
- part of the carbonaceous structure of the carbonized batch mixture body is mildly oxidized: CO 2 ( g )+C( s ) ⁇ 2CO( g ), H 2 O( g )+C( s ) ⁇ H 2 ( g )+CO( g ), resulting in the etching of the structure of the carbonaceous body and formation of an activated carbon matrix that can define a plurality of pores on a nanoscale and microscale.
- the activating conditions time, temperature and atmosphere
- the mixture may be ground or otherwise processed to form particles.
- the binder combined with the first mixture to make the second mixture is an organic resin.
- the organic resin may, for example, be cured after forming the mixture into the shape of a sorbent body. Curing can be performed, for example, according to the procedures outlined previously.
- the second mixture can then be formed into the shape of a sorbent body by any appropriate technique, such as by extrusion.
- the formed body may also be dried and optionally fired as well under conditions detailed previously.
- Sorbent bodies of the invention may be prepared by any other appropriate techniques.
- sorbents of the invention could be made by dip-coating or spraying bodies formed of bound activated carbon particles with appropriate solutions or suspensions of sulfur and/or catalyst metal.
- mixtures that are to be formed into sorbent bodies of the invention may be in the form of batch compositions that comprise:
- sulfur in any oxidation state, as elemental sulfur or in a chemical compound or moiety comprising sulfur
- a metal catalyst in any oxidation state, as elemental metal or in a chemical compound or moiety comprising the metal
- Such batch compositions may be in the form of, for example, a slurry or a paste.
- the mixtures that are to be formed into sorbent bodies in either of the methods mentioned above may also optionally comprise forming aids.
- forming aids include soaps, fatty acids, such as oleic, linoleic acid, sodium stearate, etc., polyoxyethylene stearate, etc. and combinations thereof.
- Other additives that can be useful for improving the extrusion and curing characteristics of the batch are phosphoric acid and oil.
- Exemplary oils include petroleum oils with molecular weights from about 250 to 1000, containing paraffinic and/or aromatic and/or alicyclic compounds. Some useful oils are 3 in 1 oil from 3M Co., or 3 in 1 household oil from Reckitt and Coleman Inc., Wayne, N.J.
- oils can include synthetic oils based on poly(alpha olefins), esters, polyalkylene glycols, polybutenes, silicones, polyphenyl ether, CTFE oils, and other commercially available oils.
- Vegetable oils such as sunflower oil, sesame oil, peanut oil, soyabean oil etc. are also useful.
- Sorbent bodies comprising activated carbon particles, sulfur and metal catalyst may be useful for the sorption of contaminants from a fluid.
- a further embodiment of the invention is a method for removing a contaminant from a fluid, which comprises:
- a sorbent comprising:
- Exemplary sorbents include any of those described previously as embodiments of sorbents of the present invention.
- a fluid may be contacted with a sorbent body, such as passed through a sorbent such as a honeycomb, to remove a contaminant in the fluid.
- the fluid may be in the form of a gas or a liquid.
- the gas or liquid may also contain another phase, such as a solid particulate in either a gas or liquid stream, or droplets of liquid in a gas stream.
- Example gas streams include coal combustion flue gases (such as from bituminous and sub-bituminous coal types or lignite coal) and syngas streams produced in a coal gasification process.
- sorb refers to the adsorption, absorption, or other entrapment of the contaminant on the sorbent, either physically, chemically, or both physically and chemically.
- Contaminants to be sorbed include, for instance, contaminants at 3 wt % or less within the fluid stream, for example at 2 wt % or less, or 1 wt % or less. Contaminants may also include, for instance, contaminants at 10,000 ⁇ g/m 3 or less within the fluid stream.
- Example contaminants include metals, including toxic metals.
- the term “metal” in this context and any reference to a particular metal or other contaminant by name in this context includes the elemental forms as well as oxidation states of the metal or other contaminant. Sorption of a metal or other named contaminant thus includes sorption of the elemental form of the metal or other contaminant as well as sorption of any organic or inorganic compound or composition comprising the metal or other contaminant.
- Example metals that can be sorbed include cadmium, mercury, chromium, lead, barium, beryllium, and chemical compounds or compositions comprising those elements.
- the metal is mercury in an elemental (Hg 0 ) or oxidized state (Hg + or Hg 2+ ).
- Example forms of oxidized mercury include HgO and halogenated mercury, for example Hg 2 Cl 2 and HgCl 2 .
- Other exemplary metallic contaminants include nickel, cobalt, vanadium, zinc, copper, manganese, antimony, silver, and thallium, as well as organic or inorganic compounds or compositions comprising them. Additional contaminants include arsenic and selenium as elements and in any oxidation states, including organic or inorganic compounds or compositions comprising arsenic or selenium.
- the contaminant may be in any phase that can be sorbed on the sorbent bodies.
- the contaminant may be present, for example, as a liquid in a gas fluid steam, or as a liquid in a liquid fluid stream.
- the contaminant could alternatively be present as a gas phase contaminant in a gas or liquid fluid stream.
- the contaminant is mercury vapor in a coal combustion flue gas or syngas stream.
- Activated carbon 51 wt %, sulfur powder 6 wt %, manganese dioxide powder 6 wt %, talc 30 wt %, methylcellulose 6 wt % and sodium stearate lubricant 1 wt % were mixed with water in a muller. The mixture was extruded into 100/17 honeycombs. The honeycombs were then fired to 1000° C. in nitrogen. Excellent quality honeycombs were obtained from this type of batch.
- phenolic resin as an organic binder is used to form an extruded body.
- a composition containing 61 wt % activated carbon, 6 wt % sulfur powder, 6 wt % manganese dioxide powder, 6 wt % methocel, 1 wt % sodium stearate, 20 wt % phenolic resole resin were mixed with additional water and extruded into a honeycomb structure. These honeycomb was then dried and cured at 150° C. The honeycomb may be used as cured or may be fired to a higher temperature to attain higher strength.
- an activated carbon powder was obtained as follows. Phenolic resin (39.5 wt %), charcoal (37.5 wt %), sulfur (7.1 wt %), MnO 2 (7.1 wt %), Methocel A4M (5.6 wt %), oil (2.5 wt %), and SAN (1 wt %) were mixed. The mixture was then cured at 150° C., ground to powder, and then carbonized in nitrogen at 800° C. and activated in CO 2 at 850° C. to obtain carbon powder containing sulfur and metallic catalyst and a surface area of ⁇ 850 m 2 /g.
- an activated carbon powder was obtained by mixing 45 wt % phenolic resin, 40 wt % charcoal, 7.5 wt % sulfur and 7.5 wt % MnO 2 , curing the mixture, grinding the mixture to a fine powder, and activating to obtain powder with a surface area of 900 m 2 /g.
- Composition 3 In a third technique, an activated carbon powder 85 wt % phenolic resin, 7.5 wt % sulfur and 7.5 wt % MnO 2 were mixed and treated as described above in the second technique to obtain high surface area carbon powder with sulfur and metallic catalyst.
- the three powders described above can be extruded into a honeycomb shape.
- Bentonite clay at 15 wt %, Methocel at 7 wt %, SAN at 1 wt % and 77 wt % of Composition 1 were mixed with water to make an extrudable paste.
- the mixture was extruded into a honeycomb shape and dried at 120° C.
- the honeycombs thus obtained were strong.
- Some of the honeycombs were heat treated at 800-900° C. in nitrogen. These honeycombs also were strong. Methocel was removed due to the high temperature heat treatment.
- bentonite clay at 15 wt %, SAN at 1 wt %, cellulose fiber at 7 wt %, Methocel at 7% and Composition 1 at 70 wt % were mixed, water added to make an extrudable batch and the mixture was extruded into a carbon honeycomb with excellent extrusions and good quality honeycombs after drying and heat treatment.
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Abstract
Description
-
- activated carbon particles,
- sulfur, in any oxidation state, as elemental sulfur or in a chemical compound or moiety comprising sulfur,
- a metal catalyst, in any oxidation state, as elemental metal or in a chemical compound or moiety comprising the metal, and
- a binder; and
-
- a carbon source,
- sulfur, in any oxidation state, as elemental sulfur or in a chemical compound or moiety comprising sulfur,
- a metal catalyst, in any oxidation state, as elemental metal or in a chemical compound or moiety comprising the metal, and
CO2(g)+C(s)→2CO(g),
H2O(g)+C(s)→H2(g)+CO(g),
resulting in the etching of the structure of the carbonaceous body and formation of an activated carbon matrix that can define a plurality of pores on a nanoscale and microscale. The activating conditions (time, temperature and atmosphere) can be adjusted to produce the final product with the desired specific area.
-
- activated carbon particles;
- sulfur, in any oxidation state, as elemental sulfur or in a chemical compound or moiety comprising sulfur; and
- a metal catalyst, in any oxidation state, as elemental metal or in a chemical compound or moiety comprising the metal; and
Claims (22)
Priority Applications (2)
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US12/167,418 US8691722B2 (en) | 2008-07-03 | 2008-07-03 | Sorbent comprising activated carbon particles, sulfur and metal catalyst |
PCT/US2009/003870 WO2010002444A2 (en) | 2008-07-03 | 2009-06-30 | Sorbent comprising activated carbon particles, sulfur and metal catalyst |
Applications Claiming Priority (1)
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US12/167,418 US8691722B2 (en) | 2008-07-03 | 2008-07-03 | Sorbent comprising activated carbon particles, sulfur and metal catalyst |
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US20100004119A1 US20100004119A1 (en) | 2010-01-07 |
US8691722B2 true US8691722B2 (en) | 2014-04-08 |
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US12/167,418 Expired - Fee Related US8691722B2 (en) | 2008-07-03 | 2008-07-03 | Sorbent comprising activated carbon particles, sulfur and metal catalyst |
Country Status (2)
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US (1) | US8691722B2 (en) |
WO (1) | WO2010002444A2 (en) |
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